CN116169266A - Self-doped N, S reed-based hard carbon sodium-electricity negative electrode material and preparation method thereof - Google Patents
Self-doped N, S reed-based hard carbon sodium-electricity negative electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a reed-based hard carbon sodium-electricity negative electrode material self-doped with N, S and a preparation method thereof, which belong to the technical field of sodium ion battery materials, and the preparation of the reed-based hard carbon negative electrode material self-doped with N, S is realized by a two-step carbonization method, wherein the preparation method mainly comprises the following steps: washing the dried reed with pure water, drying, crushing and sieving, pyrolyzing the raw materials at a lower temperature, performing high-temperature secondary pyrolysis on the pyrolyzed material in a closed container, and crushing and sieving to obtain the reed-based hard carbon anode material doped with N, S. The preparation method disclosed by the invention is simple in process, low in cost, green and low in carbon, and the prepared hard carbon anode material is excellent in electrochemical performance and has a better commercialized prospect.
Description
Technical Field
The invention belongs to the technical field of sodium ion battery manufacturing, and particularly relates to a reed-based hard carbon sodium-electricity negative electrode material self-doped with N, S and a preparation method thereof.
Background
Sodium has advantages such as uniform resource distribution, abundant reserves, and low price compared to lithium, and thus sodium ion batteries (NIBs) have received much attention. The conventional graphite negative electrode, which has been widely used in LIBs, is difficult to be used in the NIBs due to the fact that the interlayer spacing is small and the diameter of sodium ions is larger than that of lithium ions. Compared with graphite materials, the hard carbon materials have larger graphite interlayer spacing and more defect structures, so that sodium ions with larger ion radius can be embedded and extracted in the hard carbon materials, and meanwhile, a large number of active sites can be provided for sodium storage at defect positions. At present, the manufacturing sources of the hard carbon are mostly from high polymer materials and biomasses, wherein the biomass is adopted as the raw material of the hard carbon, and the biomass is a low-cost, green and low-carbon hard carbon preparation path.
The Chinese patent application with the prior art publication number of CN112441573A discloses a preparation method of a biomass-based hard carbon doped material, which utilizes the phoenix tree bark to successfully prepare the F-doped hard carbon material in the atmosphere of fluorine gas, so that the specific capacity of the hard carbon negative electrode material is improved. However, the synthesis of this method in toxic and irritating gases containing fluorine limits the mass production and use of hard carbon negative electrode products. Another chinese patent of technical publication No. CN115528232a uses concentrated phosphoric acid and rubber H pore-forming agent to pyrolyze reed under nitrogen atmosphere to obtain P 2 O 5 The method needs more reagents, and the concentrated phosphoric acid is easy to volatilize and has certain irritation, so that the method has larger limit on the large-scale production of the hard carbon. The method is to reserve P 2 O 5 Composite dopingThe method has the advantages that the pyrolysis is directly carried out without washing after the acid leaching of the concentrated phosphoric acid, and the phosphoric acid mixed with reed can have strong corrosion on a hearth in the pyrolysis temperature rising process, so that the service life of equipment is shortened, and the production cost is increased. In addition, phosphoric acid corrodes the furnace and can have certain impurity to drop in the pyrolysis process, easily mixes in the carbon dust, has certain influence to product purity.
Reed contains a large amount of cellulose, lignin and hemicellulose, and is often used as raw materials for papermaking in the past, but due to the continuous promotion of environmental protection policies in recent years, the scale of papermaking enterprises is continuously reduced, so that large-area waste recovery of the reed occurs, and resources cannot be fully utilized. Meanwhile, the reed can release N-containing and S-containing gases in the calcining process, and the gas is used as an N source and an S source, so that the doping of heterogeneous elements can be finished while the hard carbon is prepared. Therefore, the invention explores a reed-based hard carbon sodium-electricity negative electrode material self-doped with N, S and a preparation method thereof.
Disclosure of Invention
Based on the analysis, the primary purpose of the invention is to provide a reed-based hard carbon sodium-electricity negative electrode material of self-doping N, S and a preparation method thereof, wherein N and S-containing gas generated by high-temperature pyrolysis of reed is utilized for self-doping to prepare N and S co-doped hard carbon negative electrode material, and the prepared hard carbon negative electrode material has larger interlayer spacing, effectively improves sodium storage capacity of hard carbon, and finally improves electrochemical performance of the material.
The aim of the invention is realized by the following technical scheme: the reed-derived hard carbon sodium-electricity negative electrode material is prepared from reed as a raw material, wherein the hard carbon material is an N and S co-doped hard carbon negative electrode material and comprises C, O, N, S elements.
A preparation method of a self-doped N, S reed-based hard carbon sodium-electricity negative electrode material comprises the following steps:
(1) Eluting impurities from reed biomass by pure water, and then placing the reed biomass in a forced air drying oven for drying treatment, wherein the drying temperature is 80-110 ℃ and the drying time is 12-24 hours.
(2) Pulverizing and sieving dry reed.
(3) Pre-pyrolyzing the crushed reed at a certain temperature under a protective atmosphere, and then acid leaching and impurity removal to obtain pre-pyrolyzed carbon powder.
(4) And (3) placing the preheated carbon powder in a sealed container, carrying out final pyrolysis carbonization at a certain temperature, and after carbonization, crushing and sieving to obtain the final product, namely the self-doped N, S reed-based hard carbon anode material.
Further, the reed in the step (1) comprises one or more of dune reeds, swamp reeds, transition zone reeds and salinized meadow reeds.
Further, the mesh number of the screen in the step (2) is 50-200 mesh.
Further, in the step (3), the temperature is 400-800 ℃, and the protective atmosphere is Ar or N 2 。
Further, the acid leaching reagent in the step (3) is one or more of hydrochloric acid, sulfuric acid, phosphoric acid and hydrofluoric acid, the acid leaching time is 2-8h, and the acid leaching temperature is 30-50 ℃.
Further, the temperature in the step (4) is 1000-1600 ℃.
Further, in the step (4), the closed container is one of a graphite crucible, a corundum crucible and a porcelain crucible with a bolt cover.
In addition, when the prepared silicon-carbon composite material is used for preparing a sodium ion battery, a reed-based hard carbon anode material which is self-doped with N, S is taken as an anode active material, the anode active material is mixed with PVDF and carbon black according to a mass ratio of 8:1:1, deionized water/N-methylpyrrolidone (NMP) is taken as a solvent to be ground into uniform slurry, the uniform slurry is coated on an aluminum foil, the aluminum foil is dried in a vacuum oven at 80 ℃, and a hard carbon material electrode plate is obtained by cutting on a sheet punching machine. The obtained electrode is used as a negative electrode, a sodium sheet is used as a positive electrode, and an electrolyte is NaClO with the concentration of 1mol/L 4 A solution dissolved in ethyl carbonate/propylene carbonate (EC: pc=1:1vol%) was used as an electrolyte, and a button cell was assembled in a glove box filled with argon (Ar).
The invention has the beneficial effects that:
(1) The waste reed biomass material adopted by the invention has wide sources, and can avoid environmental pollution caused by spoilage of the reed while realizing high added value utilization of the reed.
(2) According to the invention, N and S doping is carried out on the hard carbon material simultaneously by utilizing N-containing gas and S-containing gas (volume concentration is 1%) generated by reed biomass body pyrolysis in a closed high-temperature process, and finally N, S co-doped hard carbon material can be successfully prepared; and cracking gas generated in the conventional open high-temperature process flows out of the furnace along with the protective inert atmosphere, so that N and S doping cannot be carried out on the hard carbon material.
(3) The invention and the same type of patent P 2 O 5 Compared with the composite nitrogen-doped reed-based porous hard carbon anode material, the preparation method disclosed by the invention has the advantages of simple process, short flow, low raw material price, no need of adding additional reagents, effective utilization of tail gas generated in the high-temperature calcination process, easiness in realization of mass production and better commercialization prospect.
(3) The invention and the same type of patent P 2 O 5 Compared with the composite nitrogen-doped reed-based porous hard carbon anode material, the invention has less corrosion to the hearth in the high-temperature transformation process, and does not need to consider the influence of the impurity falling in the hearth corrosion process on the purity of the hard carbon anode.
(4) The specific capacity of the hard carbon anode material prepared under the optimized condition of the invention can reach about 390 mA.h/g, which is similar to the patent P 2 O 5 Compared with the composite nitrogen-doped reed-based porous hard carbon negative electrode material, the hard carbon negative electrode has remarkable specific capacity improving effect.
(5) The invention and the same type of patent P 2 O 5 Compared with the composite nitrogen-doped reed-based porous hard carbon anode material, the preparation method disclosed by the invention does not need additional toxic and harmful gases for doping, and meanwhile, the original waste tail gas can be fully utilized in a closed reaction environment, so that the negative influence on production equipment is avoided, and the preparation method belongs to an environment-friendly hard carbon material preparation method.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
FIG. 1 is an SEM image of the product of embodiment 1 of the invention.
Figure 2 shows the XRD results of the product of example 1 of the present invention.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
Eluting 50g of reed with pure water, drying at 90 ℃ for 24 hours, crushing, sieving, crushing reed to 100 meshes, placing the reed in a tubular furnace (Ar atmosphere) for pyrolysis at 500 ℃ for 2 hours, and removing impurities from the pyrolyzed carbon material in hydrofluoric acid at 40 ℃ to obtain preheated carbon powder. And (3) placing the preheated carbon powder in a sealed corundum crucible, then placing the sealed corundum crucible in a tube furnace (Ar atmosphere) for carbonization for 2 hours at 1300 ℃, and grinding and screening the finally carbonized product to obtain the self-doped N, S reed-based hard carbon anode material, wherein the N content is 2.05% and the S content is 1.04%.
The SEM image of the hard carbon anode material prepared by the embodiment is shown in fig. 1, the hard carbon material maintains the original structure of the reed biomass material, has a large number of pore channels, can be used for sodium ion transmission and storage, and shows that the material can be embedded with more sodium ions.
As shown in figure 2, the XRD pattern of the material is shown in figure 2, the prepared carbon material is an amorphous hard carbon material, wherein about 22 degrees of the carbon material has a wide peak, corresponding to the (002) plane of a graphite crystal form, about 43 degrees of the carbon material also has a wide peak, corresponding to the (100) plane of the graphite crystal form, and meanwhile, no obvious impurity peak in the pattern indicates that the effect of removing impurities in the hard carbon is better.
The reed-based hard carbon anode material self-doped with N, S is taken as an anode active material, mixed with PVDF and carbon black according to the mass ratio of 8:1:1, ground into uniform slurry by taking deionized water/N-methylpyrrolidone (NMP) as a solvent, coated on an aluminum foil, dried in a vacuum oven at 80 ℃ and then punched into a sheet machineAnd (5) cutting the upper piece to obtain the hard carbon material electrode piece. The obtained electrode is used as a negative electrode, a sodium sheet is used as a positive electrode, and an electrolyte is NaClO with the concentration of 1mol/L 4 A solution dissolved in ethyl carbonate/propylene carbonate (EC: pc=1:1vol%) was used as an electrolyte, and a button cell was assembled in a glove box filled with argon (Ar). The reversible capacity of the assembled battery at the rate of 0.5C is 393.1 mA.h/g.
Comparative example 1
Eluting 50g of reed with pure water, drying at 90 ℃ for 24 hours, crushing, sieving, crushing reed to 100 meshes, placing the reed in a tubular furnace (Ar atmosphere) for pyrolysis at 500 ℃ for 2 hours, and removing impurities from the pyrolyzed carbon material in hydrofluoric acid at 40 ℃ to obtain preheated carbon powder. And (3) placing the preheated carbon powder in an open corundum crucible, then placing the open corundum crucible in a tubular furnace (Ar atmosphere) for carbonization at 1300 ℃ for 2 hours, and grinding and screening the finally carbonized product to obtain the self-doped N, S reed-based hard carbon anode material, wherein the N content is 0.08% and the S content is 0.02%.
The battery was assembled in the same manner as in example 1. The reversible capacity of the assembled battery at the rate of 0.5C is 230.7mA.h/g.
Example 2
Eluting 50g of reed with pure water, drying at 90 ℃ for 24 hours, crushing, sieving, crushing reed to 100 meshes, placing the reed in a tubular furnace (Ar atmosphere) for pyrolysis at 600 ℃ for 2 hours, and removing impurities from the pyrolyzed carbon material in hydrofluoric acid at 40 ℃ to obtain preheated carbon powder. And (3) placing the preheated carbon powder in a sealed corundum crucible, then placing the sealed corundum crucible in a tube furnace (Ar atmosphere) for carbonization for 2 hours at 1300 ℃, and grinding and screening the finally carbonized product to obtain the self-doped N, S reed-based hard carbon anode material, wherein the N content is 1.38% and the S content is 0.63%.
The battery was assembled in the same manner as in example 1. The reversible capacity of the assembled battery at the rate of 0.5C is 351 mA.h/g.
Example 3
Eluting 50g of reed with pure water, drying at 90 ℃ for 24 hours, crushing, sieving, crushing reed to 100 meshes, placing the reed in a tubular furnace (Ar atmosphere) for pyrolysis at 800 ℃ for 2 hours, and removing impurities from the pyrolyzed carbon material in hydrofluoric acid at 40 ℃ to obtain preheated carbon powder. And (3) placing the preheated carbon powder in a sealed corundum crucible, then placing the sealed corundum crucible in a tube furnace (Ar atmosphere) for carbonization for 2 hours at 1300 ℃, and grinding and screening the finally carbonized product to obtain the self-doped N, S reed-based hard carbon anode material, wherein the N content is 0.96% and the S content is 0.34%.
The battery was assembled in the same manner as in example 1. The reversible capacity of the assembled battery at the rate of 0.5C is 328.8 mA.h/g.
Example 4
The final pyrolysis temperature for preparing the hard carbon material is 1000 ℃, the rest process parameters are the same as those of the example 1, and the obtained hard carbon material has the N content of 1.26% and the S content of 0.54%.
The battery was assembled in the same manner as in example 1. The reversible capacity of the assembled battery at the rate of 0.5C is 313.6mA.h/g.
Example 5
The final pyrolysis temperature for preparing the hard carbon material is 1200 ℃, and the rest process parameters are the same as those of the example 1, wherein the content of N in the obtained hard carbon material is 1.64%, and the content of S is 0.87%.
The battery was assembled in the same manner as in example 1. The reversible capacity of the assembled battery at the rate of 0.5C is 346.7 mA.h/g.
Example 6
The final pyrolysis temperature for preparing the hard carbon material is 1400 ℃, and the rest process parameters are the same as those of the example 1, wherein the content of N in the obtained hard carbon material is 2.56%, and the content of S is 1.65%.
The battery was assembled in the same manner as in example 1. The reversible capacity of the assembled battery at the rate of 0.5C is 362.2 mA.h/g.
The performance comparison summary of the above examples and comparative examples is shown below:
in summary, when reed is crushed to 100 meshes, the pre-pyrolysis temperature is 500 ℃, and the final pyrolysis temperature is 1300 ℃, the prepared self-doped N, S reed-based hard carbon anode material has the best performance.
The above description is only a basic description of the inventive concept, and any equivalent transformation according to the technical solution of the present invention shall fall within the protection scope of the present invention.
Claims (9)
1. The reed-based hard carbon sodium-electricity negative electrode material of self-doping N, S is characterized in that the hard carbon material is prepared from reed as a raw material, is a porous hard carbon material doped with nitrogen and sulfur, and comprises C, O, N, S elements.
2. A method for preparing the self-doped N, S reed-based hard carbon sodium electric negative electrode material according to claim 1, comprising the following steps:
(1) Eluting impurities from reed biomass by pure water, and then placing the reed biomass in a forced air drying oven for drying treatment, wherein the drying temperature is 80-110 ℃ and the drying time is 12-24 hours;
(2) Crushing and sieving the dried reed;
(3) Pre-pyrolyzing the crushed reed at a certain temperature under a protective atmosphere, and then acid leaching and impurity removal to obtain pre-pyrolyzed carbon powder;
(4) And (3) placing the preheated carbon powder in a sealed container, carrying out final pyrolysis carbonization at a certain temperature, and after carbonization, crushing and sieving to obtain the final product, namely the self-doped N, S reed-based hard carbon anode material.
3. The method of claim 2, wherein the reed in step (1) comprises one or more of dune reed, swamp reed, transition zone reed and salinized meadow reed.
4. The method for preparing a reed-based hard carbon sodium electric negative electrode material self-doping N, S as set forth in claim 2, wherein the mesh number of the screen in the step (2) is 50-200 mesh.
5. The method for preparing the self-doping N, S reed-based hard carbon sodium electric negative electrode material according to claim 2, wherein in the step (3), the temperature is 400-800 ℃, and the protective atmosphere is Ar or N 2 。
6. The method for preparing the self-doping N, S reed-based hard carbon sodium electric negative electrode material according to claim 2, wherein the acid leaching reagent in the step (3) is one or more of hydrochloric acid, sulfuric acid, phosphoric acid and hydrofluoric acid, the acid leaching time is 2-8h, and the acid leaching temperature is 30-50 ℃.
7. The method for preparing a self-doping N, S reed-based hard carbon sodium electronegative electrode material according to claim 2, wherein the temperature in the step (4) is 1000-1600 ℃.
8. The method for preparing the self-doping N, S reed-based hard carbon sodium electric negative electrode material according to claim 2, wherein the closed container in the step (4) is one of a graphite crucible with a bolt cover, a corundum crucible and a porcelain crucible.
9. The use of the hard carbon negative electrode material according to claim 8 in a negative electrode of a sodium ion battery.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116979064A (en) * | 2023-09-25 | 2023-10-31 | 宁德时代新能源科技股份有限公司 | Carbon material and preparation method thereof, negative electrode plate, secondary battery and power utilization device |
| CN116995230A (en) * | 2023-09-25 | 2023-11-03 | 宁德时代新能源科技股份有限公司 | Carbon material and preparation method thereof, negative electrode plate, secondary battery and power utilization device |
| CN116995231A (en) * | 2023-09-25 | 2023-11-03 | 宁德时代新能源科技股份有限公司 | Carbon material and preparation method thereof, negative electrode plate, secondary battery and power utilization device |
| CN117832482A (en) * | 2024-03-06 | 2024-04-05 | 碳一新能源(杭州)有限责任公司 | Nitrogen-doped hard carbon material, preparation method thereof, negative plate, sodium ion battery and application |
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| CN116979064A (en) * | 2023-09-25 | 2023-10-31 | 宁德时代新能源科技股份有限公司 | Carbon material and preparation method thereof, negative electrode plate, secondary battery and power utilization device |
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| CN116995231B (en) * | 2023-09-25 | 2024-04-09 | 宁德时代新能源科技股份有限公司 | Carbon material and preparation method thereof, negative electrode plate, secondary battery and power utilization device |
| CN116995230B (en) * | 2023-09-25 | 2024-04-09 | 宁德时代新能源科技股份有限公司 | Carbon material and preparation method thereof, negative electrode plate, secondary battery and power utilization device |
| CN117832482A (en) * | 2024-03-06 | 2024-04-05 | 碳一新能源(杭州)有限责任公司 | Nitrogen-doped hard carbon material, preparation method thereof, negative plate, sodium ion battery and application |
| CN117865127A (en) * | 2024-03-11 | 2024-04-12 | 钛科(大连)新能源有限公司 | Cotton straw-based biomass hard carbon anode material and preparation method and application thereof |
| CN117865127B (en) * | 2024-03-11 | 2024-05-17 | 钛科(大连)新能源有限公司 | Cotton straw-based biomass hard carbon anode material and preparation method and application thereof |
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